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Piperidine → HCID 20505900, 화합물

HRID 1390511
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HRID 1390511 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11](Cl)(=[O:13])=[O:12])=[C:7]([Cl:15])[C:3]=1[C:4]([OH:6])=[O:5].[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>C(Cl)Cl>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11]([N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)(=[O:13])=[O:12])=[C:7]([Cl:15])[C:3]=1[C:4]([OH:6])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8082PiperidineHCID 35382162,6-Dichloro-3-(chlorosulfonyl)benzoic acid

생성물 1

HCID 20505900HCID 20505900, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2,6-Dichloro-5-chlorosulfonylbenzoic acid (960 mg.; 3.3 m moles) is added portion-wise to 1.95 g. (0.0165 mole) of piperidine in 15 ml. of dry methylene chloride, and the mixture heated to reflux for 1.5 hrs. The solvent and excess amine are removed under reduced pressure and the residue dissolved in 15 ml. of 2N sodium hydroxide. The aqueous base solution is extracted (2 × 50 ml.) with ether and acidified with 6N hydrochloric acid. The precipitated gum is filtered, dried and allowed to crystallize in hexane, 1.1 g., m.p. 145°-150° C. A small sample is recrystallized from acetonitrile, m.p. 142°-145° C.

후처리

  1. temperatureto reflux for 1.5 hrs
  2. customThe solvent and excess amine are removed under reduced pressure
  3. dissolutionthe residue dissolved in 15 ml
  4. extractionThe aqueous base solution is extracted (2 × 50 ml.) with ether
  5. filtrationThe precipitated gum is filtered
  6. customdried
  7. customto crystallize in hexane
  8. customA small sample is recrystallized from acetonitrile, m.p. 142°-145° C.

출처 및 근거

ORD 기록
ord-b5414fb9ad564cb1bce06d308d1f182d
출처 데이터셋
uspto-grants-1979_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04138399

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